US11577215B2 - Method for producing absorbent - Google Patents

Method for producing absorbent Download PDF

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US11577215B2
US11577215B2 US17/472,619 US202117472619A US11577215B2 US 11577215 B2 US11577215 B2 US 11577215B2 US 202117472619 A US202117472619 A US 202117472619A US 11577215 B2 US11577215 B2 US 11577215B2
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adsorbent
wastewater
hexametaphosphate
titanium
thallium
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US20220126265A1 (en
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Gaosheng Zhang
Ye Liu
Huosheng LI
Xiangping Li
Yongheng CHEN
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Guangzhou University
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Guangzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0211—Compounds of Ti, Zr, Hf
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3071—Washing or leaching
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the disclosure relates to a field of wastewater treatment technologies, and particularly to an adsorbent and its preparation method and application.
  • Adsorption method is one of the most efficient methods for removing thallium contaminants in underground water, surface water and industrial wastewater.
  • the method is characterized by simple operation, low cost, low sludge production, low secondary pollution risk, etc., which is generally applicable to a water treatment system with a large treatment capacity and a low contaminant concentration.
  • a solid material is configured as an adsorbent to transfer thallium contaminants from a water phase to an adsorbent surface through physical adsorption, chemical adsorption, ion exchange, etc., thereby achieving the purpose of removing thallium in water.
  • adsorbent materials for removing thallium including natural minerals, industrial and agricultural wastes and synthetic adsorbent materials.
  • Low-cost adsorbents are zeolite, montmorillonite, kaolin and cellulose; synthetic adsorbent materials are activated carbon, titanium dioxide, titanium peroxide, manganese dioxide, hydrated ferric oxide, fe-mn composite oxide, magnetic ferroferric oxide, aluminum oxide, etc.
  • the present disclosure is intended to solve at least one of technical problems existing in the related art.
  • the disclosure provides an adsorbent that may effectively treat acidic thallium-containing wastewater, with a simple preparation method and low cost.
  • An adsorbent includes titanium hexametaphosphate; the titanium hexametaphosphate is mainly prepared from hexametaphosphate and titanium salt.
  • the titanium hexametaphosphate is mainly prepared from hexametaphosphate and titanium salt under acidic conditions.
  • the particle size of the titanium hexametaphosphate is 10 nm to 10 ⁇ m.
  • a method for preparing an adsorbent includes:
  • the pH is 0-6; further preferably, the pH is 0-3.
  • a ratio of amount of substance of the hexametaphosphate to the titanium salt is (1-2):(3-1).
  • the hexametaphosphate is selected from at least one of sodium hexametaphosphate, potassium hexametaphosphate or ammonium hexametaphosphate.
  • the titanium salt is selected from at least one of titanium tetrachloride, titanium oxychloride, titanium nitrate or titanium sulfate.
  • the concentrated acid is selected from at least one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid.
  • the reaction temperature is 25° C.-180° C.; preferably, the reaction temperature is 85° C.-160° C.; more preferably, the reaction temperature is 90° C.-150° C.
  • the aging time is 1-24 h; preferably, the aging time is 8-24 h.
  • the preparation method further includes purification of a filter residue.
  • the purification method includes water washing and drying.
  • the drying process includes: drying at 40° C.-60° C. for 1-12 h, and then drying at 90-120° C. for 6-24 h; further preferably, drying at 40° C.-55° C. for 1-12 h, and then drying at 100-110° C. for 6-24 h.
  • a wastewater treatment agent includes the adsorbent.
  • the disclosure has the following beneficial effects:
  • the adsorbent is an aggregate of micron or nanometer particles, with a large surface area and a good adsorption performance.
  • the adsorbent as a wastewater treatment agent, may effectively remove thallium contaminants in various water bodies such as underground water, surface water, industrial wastewater and mine wastewater at a removal rate of 99.8%; and the adsorbent has a good removal capability for heavy metals in water such as cadmium, plumbum, copper, stibium, cesium, uranium.
  • the adsorbent has a wide applicable pH value range, and especially has a good adsorption capacity, stability and heat resistance under acidic conditions.
  • FIG. 1 is a scanning electron microscope (SEM) diagram of an adsorbent prepared in Embodiment 1;
  • FIG. 2 is an X-ray diffraction (XRD) diagram of an adsorbent prepared in Embodiment 1;
  • FIG. 3 is a scanning electron microscope (SEM) diagram of an adsorbent prepared in Embodiment 2.
  • the titanium dioxide adsorbent, the manganese dioxide adsorbent, the hydrated ferric oxide adsorbent and the aluminum oxide adsorbent in the following contrast embodiments are purchased from Beijing Top Science Biological Technology Co., Ltd.; the raw materials, reagents or apparatuses used in the following embodiments may be purchased from a conventional commercial approach, or may be obtained by a known method.
  • FIG. 1 is an SEM diagram of an adsorbent prepared in Embodiment 1, and it can be seen that titanium hexametaphosphate adsorbent-1 nanoparticles are formed by agglomeration of lamellar structures and in a pleated pattern.
  • FIG. 2 is an X-ray diffraction (XRD) diagram of a titanium hexametaphosphate adsorbent-1, and it can be obviously seen that two peaks appear at 12 degrees and 29 degrees respectively.
  • XRD X-ray diffraction
  • a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.35 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.349 mg/L and a pH of wastewater is 5.5.
  • Take 1 L wastewater add 0.45 g titanium hexametaphosphate adsorbent-1 prepared in Embodiment 1, perform solid-liquid separation after stirring and mixing for 2 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.85 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.524 mg/L and a pH of wastewater is 3.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-3 prepared in Embodiment 3, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.05 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.721 mg/L and a pH of wastewater is 2.5.
  • Take 1 L wastewater add 0.6 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.95 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.876 mg/L and a pH of wastewater is 4.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-5 prepared in Embodiment 5, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.15 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-6 prepared in Embodiment 6, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.85 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-7 prepared in Embodiment 7, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.45 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5.
  • Take 1 L wastewater add 0.5 g titanium hexametaphosphate adsorbent-8 prepared in Embodiment 8, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.95 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent thallium is 2.349 mg/L and a pH of wastewater is 5.5.
  • Take 1 L wastewater add 0.45 g titanium hexametaphosphate adsorbent-9 prepared in Embodiment 9, perform solid-liquid separation after stirring and mixing for 2 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.55 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of univalent Thallium is 2.157 mg/L and a pH of wastewater is 3.5.
  • Take 1 L wastewater add 0.8 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.35 ⁇ g/L, less than 5 ⁇ g/L.
  • a concentration of cadmiun is 15.159 mg/L and a pH of wastewater is 7.0.
  • Take 1 L wastewater add 0.8 g titanium hexametaphosphate adsorbent-5 prepared in Embodiment 5, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of cadmiun in the wastewater by an ICP-MS method, the concentration of cadmiun being 0.045 mg/L(less than 0.05 mg/L).
  • a concentration of plumbum is 4.065 mg/L and a pH of wastewater is 8.0.
  • Take 1 L wastewater add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of plumbum in the wastewater by an ICP-MS method, the concentration of plumbum in wastewater measured being 4.5 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of copper is 3.071 mg/L and a pH of wastewater is 6.5.
  • Take 1 L wastewater add 0.8 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of copper in the wastewater by an ICP-MS method, the concentration of copper in wastewater measured being 3.7 ⁇ g/L(less than 5 ⁇ g/L).
  • a concentration of stibium is 3.446 mg/L and a pH of wastewater is 7.2.
  • Take 1 L wastewater add 0.8 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of stibium in the wastewater by an ICP-MS method, the concentration of stibium in wastewater measured being 5 ⁇ g/L(less than 6 ⁇ g/L).
  • a concentration of uranium is 2.53 mg/L and a pH of wastewater is 7.5.
  • Take 1 L wastewater add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of uranium in the wastewater by an ICP-MS method, the concentration of uranium in wastewater measured being 78 ⁇ g/L(less than 0.1 mg/L).
  • a concentration of caesium is 3.653 mg/L and a pH of wastewater is 7.5.
  • Take 1 L wastewater add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of caesium in the wastewater by an ICP-MS method, the concentration of caesium in wastewater measured being 88 ⁇ g/L.
  • a concentration of thallium is 4.317 ⁇ g/L and a pH of wastewater is 2.7.
  • Take 1 L wastewater add 0.1 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 1.211 m/L.
  • a concentration of stibium is 14.876 m/L and a pH of wastewater is 2.7.
  • Take 1 L wastewater add 0.1 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of stibium in the wastewater by an ICP-MS method, the concentration of stibium in wastewater measured being 2.345 ⁇ g/L.
  • a concentration of univalent thallium is 2.157 mg/L and a pH of wastewater is 2.7.
  • Take 1 L wastewater add 0.8 g titanium dioxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 0.205 mg/L.
  • a concentration of univalent thallium is 5.029 mg/L and a pH of wastewater is 3.5.
  • Take 1 L wastewater add 0.5 g manganese dioxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.183 mg/L and the concentration of manganese being 1.211 mg/L (material dissolved).
  • a concentration of univalent thallium is 4.121 mg/L and a pH of wastewater is 3.0.
  • Take 1 L wastewater add 0.6 g hydrated ferric oxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.335 mg/L and the concentration of ferri being 2.19 mg/L (material dissolved).
  • a concentration of univalent thallium is 6.923 mg/L and a pH of wastewater is 2.7.
  • Take 1 L wastewater add 0.8 g aluminum oxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.818 mg/L and the concentration of aluminum being 0.819 mg/L (material dissolved).

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Abstract

An adsorbent for wastewater treatment includes titanium hexametaphosphate; the titanium hexametaphosphate is mainly prepared from hexametaphosphate and titanium salt. The adsorbent is an aggregate of micron or nanometer particles, with a large surface area and a good adsorption performance. The adsorbent, as a wastewater treatment agent, may effectively remove thallium contaminants in various water bodies such as underground water, surface water, chemical wastewater and mine wastewater at a removal rate of 99.8%; and the adsorbent has a good removal capability for heavy metals in water such as cadmium, plumbum, copper, stibium, cesium and uranium. The adsorbent has a wide applicable PH value range, and especially has a good adsorption capacity, stability and heat resistance under acidic conditions.

Description

TECHNICAL FIELD
The disclosure relates to a field of wastewater treatment technologies, and particularly to an adsorbent and its preparation method and application.
BACKGROUND
Adsorption method is one of the most efficient methods for removing thallium contaminants in underground water, surface water and industrial wastewater. The method is characterized by simple operation, low cost, low sludge production, low secondary pollution risk, etc., which is generally applicable to a water treatment system with a large treatment capacity and a low contaminant concentration. In the method, a solid material is configured as an adsorbent to transfer thallium contaminants from a water phase to an adsorbent surface through physical adsorption, chemical adsorption, ion exchange, etc., thereby achieving the purpose of removing thallium in water.
There are many adsorbent materials for removing thallium, including natural minerals, industrial and agricultural wastes and synthetic adsorbent materials. Low-cost adsorbents are zeolite, montmorillonite, kaolin and cellulose; synthetic adsorbent materials are activated carbon, titanium dioxide, titanium peroxide, manganese dioxide, hydrated ferric oxide, fe-mn composite oxide, magnetic ferroferric oxide, aluminum oxide, etc. Most existing thallium removal adsorbent materials have a better removal effectiveness for thallium at a pH above 7, however, the removal effectiveness is poor and the material stability is poor at a low pH. In real situations, the pH of most thallium-containing wastewater is very low (for example, a mine wastewater pH=2.7), which limits the actual application of the adsorbent material.
Therefore, it is urgent to provide an adsorbent capable of effectively treating acidic thallium-containing wastewater.
SUMMARY
The present disclosure is intended to solve at least one of technical problems existing in the related art. For this purpose, the disclosure provides an adsorbent that may effectively treat acidic thallium-containing wastewater, with a simple preparation method and low cost.
An adsorbent includes titanium hexametaphosphate; the titanium hexametaphosphate is mainly prepared from hexametaphosphate and titanium salt.
Preferably, the titanium hexametaphosphate is mainly prepared from hexametaphosphate and titanium salt under acidic conditions.
Preferably, the particle size of the titanium hexametaphosphate is 10 nm to 10 μm.
A method for preparing an adsorbent includes:
Adding acid into a hexametaphosphate solution for adjusting a pH to prepare a mixed solution, adding titanium salt into the mixed solution, reacting, aging and filtering to obtain a filter residue, namely the adsorbent.
Preferably, the pH is 0-6; further preferably, the pH is 0-3.
Preferably, a ratio of amount of substance of the hexametaphosphate to the titanium salt is (1-2):(3-1).
Preferably, the hexametaphosphate is selected from at least one of sodium hexametaphosphate, potassium hexametaphosphate or ammonium hexametaphosphate.
Preferably, the titanium salt is selected from at least one of titanium tetrachloride, titanium oxychloride, titanium nitrate or titanium sulfate.
Preferably, the concentrated acid is selected from at least one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid.
Preferably, the reaction temperature is 25° C.-180° C.; preferably, the reaction temperature is 85° C.-160° C.; more preferably, the reaction temperature is 90° C.-150° C.
Preferably, the aging time is 1-24 h; preferably, the aging time is 8-24 h.
Preferably, the preparation method further includes purification of a filter residue.
Preferably, the purification method includes water washing and drying.
Preferably, the drying process includes: drying at 40° C.-60° C. for 1-12 h, and then drying at 90-120° C. for 6-24 h; further preferably, drying at 40° C.-55° C. for 1-12 h, and then drying at 100-110° C. for 6-24 h.
A wastewater treatment agent includes the adsorbent.
The application of the adsorbent in wastewater treatment.
Compared with the related art, the disclosure has the following beneficial effects:
(1) The adsorbent is an aggregate of micron or nanometer particles, with a large surface area and a good adsorption performance. The adsorbent, as a wastewater treatment agent, may effectively remove thallium contaminants in various water bodies such as underground water, surface water, industrial wastewater and mine wastewater at a removal rate of 99.8%; and the adsorbent has a good removal capability for heavy metals in water such as cadmium, plumbum, copper, stibium, cesium, uranium.
(2) The adsorbent has a wide applicable pH value range, and especially has a good adsorption capacity, stability and heat resistance under acidic conditions.
(3) The preparation method is simple to operate, low in reaction condition requirements and low in cost.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a scanning electron microscope (SEM) diagram of an adsorbent prepared in Embodiment 1;
FIG. 2 is an X-ray diffraction (XRD) diagram of an adsorbent prepared in Embodiment 1;
FIG. 3 is a scanning electron microscope (SEM) diagram of an adsorbent prepared in Embodiment 2.
 DETAILED DESCRIPTION
To make those skilled in the art understand the technical scheme more clearly, the following embodiments are listed for illustration. It should be noted that the following embodiments are not intended to be a limitation of the protection scope of the claims.
The titanium dioxide adsorbent, the manganese dioxide adsorbent, the hydrated ferric oxide adsorbent and the aluminum oxide adsorbent in the following contrast embodiments are purchased from Beijing Top Science Biological Technology Co., Ltd.; the raw materials, reagents or apparatuses used in the following embodiments may be purchased from a conventional commercial approach, or may be obtained by a known method.
Embodiment 1: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 1; rapidly stir the solution at a room temperature, add 0.3 mol Ti(SO4)2, continue stirring for 1 h, and stand still at a room temperature to age for 24 h. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 4 times with deionized water, dry the solid filter cake in an oven at 50° C. for 2 h after separating the adsorbent, heat up to 100° C. and dry for 12 h to obtain a titanium hexametaphosphate adsorbent-1. FIG. 1 is an SEM diagram of an adsorbent prepared in Embodiment 1, and it can be seen that titanium hexametaphosphate adsorbent-1 nanoparticles are formed by agglomeration of lamellar structures and in a pleated pattern. FIG. 2 is an X-ray diffraction (XRD) diagram of a titanium hexametaphosphate adsorbent-1, and it can be obviously seen that two peaks appear at 12 degrees and 29 degrees respectively.
Embodiment 2: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 2; rapidly stir the solution at a room temperature and add 0.4 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 100° C. for 6 h. Take out and stand still at a room temperature to age for 12 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 55° C. for 8 h after separating the adsorbent, heat up to 100° C. and dry for 8 h to obtain a titanium hexametaphosphate adsorbent-2. The SEM diagram sees FIG. 3 .
Embodiment 3: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 0; rapidly stir the solution at a room temperature and add 0.5 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 150° C. for 6 h. Take out and stand still at a room temperature to age for 8 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 4 times with deionized water, dry the solid filter cake in an oven at 40° C. for 12 h after separating the adsorbent, heat up to 100° C. and dry for 6 h to obtain a titanium hexametaphosphate adsorbent-3.
Embodiment 4: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 1; rapidly stir the solution at a room temperature and add 0.6 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 85° C. for 8 h. Take out and stand still at a room temperature to age for 6 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 43° C. for 9 h after separating the adsorbent, heat up to 100° C. and dry for 20 h to obtain a titanium hexametaphosphate adsorbent.
Embodiment 5: Preparation of an Adsorbent
Weigh 0.4 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 1; rapidly stir the solution at a room temperature and add 0.2 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 180° C. for 8 h. Take out and stand still at a room temperature to age for 6 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 43° C. for 9 h after separating the adsorbent, heat up to 120° C. and dry for 12 h to obtain a titanium hexametaphosphate adsorbent.
Embodiment 6: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 4; rapidly stir the solution at a room temperature and add 0.4 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 100° C. for 6 h. Take out and stand still at a room temperature to age for 12 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 55° C. for 8 h after separating the adsorbent, heat up to 100° C. dry for 8 h to obtain a titanium hexametaphosphate adsorbent-6.
Embodiment 7: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated sulfuric acid to adjust the pH of the solution to 2; rapidly stir the solution and add 0.4 mol titanium tetrachloride. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 100° C. for 6 h. Take out and stand still at a room temperature to age for 12 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 55° C. for 8 h after separating the adsorbent, heat up to 100° C. dry for 8 h to obtain a titanium hexametaphosphate adsorbent-7.
Embodiment 8: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 2; rapidly stir the solution at a room temperature and add 0.4 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 100° C. for 6 h. Take out and stand still at a room temperature to age for 12 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 3 times with deionized water, dry the solid filter cake in an oven at 85° C. for 16 h after separating the adsorbent to obtain a titanium hexametaphosphate adsorbent-8.
Embodiment 9: Preparation of an Adsorbent
Weigh 0.2 mol (NaPO3)6 and dissolve in 200 mL water to prepare a solution; add concentrated nitric acid to adjust the pH of the solution to 1; rapidly stir the solution at a room temperature and add 0.3 mol Ti(SO4)2. Then pour a mixture into a reactor and continue a hydrothermal reaction in an oven at 100° C. for 1 h. Take out and stand still at a room temperature to age for 24 h after completion. Pour out above water, then add 1000 mL deionized water, stir and wash for 10 min, perform solid-liquid separation by a suction filtration method, continue washing a solid filter cake for 4 times with deionized water, dry the solid filter cake in an oven at 50° C. for 2 h after separating the adsorbent, heat up to 100° C. dry for 12 h to obtain a titanium hexametaphosphate adsorbent-9.
Embodiment 10: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.35 μg/L(less than 5 μg/L).
Embodiment 11: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.349 mg/L and a pH of wastewater is 5.5. Take 1 L wastewater, add 0.45 g titanium hexametaphosphate adsorbent-1 prepared in Embodiment 1, perform solid-liquid separation after stirring and mixing for 2 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.85 μg/L(less than 5 μg/L).
Embodiment 12: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.524 mg/L and a pH of wastewater is 3.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-3 prepared in Embodiment 3, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.05 μg/L(less than 5 μg/L).
Embodiment 13: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.721 mg/L and a pH of wastewater is 2.5. Take 1 L wastewater, add 0.6 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.95 μg/L(less than 5 μg/L).
Embodiment 14: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.876 mg/L and a pH of wastewater is 4.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-5 prepared in Embodiment 5, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.15 μg/L(less than 5 μg/L).
Embodiment 15: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-6 prepared in Embodiment 6, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.85 μg/L(less than 5 μg/L).
Embodiment 16: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-7 prepared in Embodiment 7, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.45 μg/L(less than 5 μg/L).
Embodiment 17: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.029 mg/L and a pH of wastewater is 6.5. Take 1 L wastewater, add 0.5 g titanium hexametaphosphate adsorbent-8 prepared in Embodiment 8, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 4.95 μg/L(less than 5 μg/L).
Embodiment 18: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.349 mg/L and a pH of wastewater is 5.5. Take 1 L wastewater, add 0.45 g titanium hexametaphosphate adsorbent-9 prepared in Embodiment 9, perform solid-liquid separation after stirring and mixing for 2 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.55 μg/L(less than 5 μg/L).
Embodiment 19: Application of an Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent Thallium is 2.157 mg/L and a pH of wastewater is 3.5. Take 1 L wastewater, add 0.8 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 3.35 μg/L, less than 5 μg/L.
Embodiment 20: Application of an Adsorbent in Wastewater Treatment
For certain cadmiun-containing wastewater, a concentration of cadmiun is 15.159 mg/L and a pH of wastewater is 7.0. Take 1 L wastewater, add 0.8 g titanium hexametaphosphate adsorbent-5 prepared in Embodiment 5, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of cadmiun in the wastewater by an ICP-MS method, the concentration of cadmiun being 0.045 mg/L(less than 0.05 mg/L).
Embodiment 21: Application of an Adsorbent in Wastewater Treatment
For certain plumbum-containing wastewater, a concentration of plumbum is 4.065 mg/L and a pH of wastewater is 8.0. Take 1 L wastewater, add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of plumbum in the wastewater by an ICP-MS method, the concentration of plumbum in wastewater measured being 4.5 μg/L(less than 5 μg/L).
Embodiment 22: Application of an Adsorbent in Wastewater Treatment
For certain copper-containing wastewater, a concentration of copper is 3.071 mg/L and a pH of wastewater is 6.5. Take 1 L wastewater, add 0.8 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of copper in the wastewater by an ICP-MS method, the concentration of copper in wastewater measured being 3.7 μg/L(less than 5 μg/L).
Embodiment 23: Application of an Adsorbent in Wastewater Treatment
For certain stibium-containing wastewater, a concentration of stibium is 3.446 mg/L and a pH of wastewater is 7.2. Take 1 L wastewater, add 0.8 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of stibium in the wastewater by an ICP-MS method, the concentration of stibium in wastewater measured being 5 μg/L(less than 6 μg/L).
Embodiment 24: Application of an Adsorbent in Wastewater Treatment
For certain uranium-containing wastewater, a concentration of uranium is 2.53 mg/L and a pH of wastewater is 7.5. Take 1 L wastewater, add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of uranium in the wastewater by an ICP-MS method, the concentration of uranium in wastewater measured being 78 μg/L(less than 0.1 mg/L).
Embodiment 25: Application of an Adsorbent in Wastewater Treatment
For certain caesium-containing wastewater, a concentration of caesium is 3.653 mg/L and a pH of wastewater is 7.5. Take 1 L wastewater, add 1.0 g titanium hexametaphosphate adsorbent-4 prepared in Embodiment 4, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of caesium in the wastewater by an ICP-MS method, the concentration of caesium in wastewater measured being 88 μg/L.
Embodiment 26: Application of an Adsorbent in Wastewater Treatment
For certain acid mine wastewater, a concentration of thallium is 4.317 μg/L and a pH of wastewater is 2.7. Take 1 L wastewater, add 0.1 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 1.211 m/L.
Embodiment 27: Application of an Adsorbent in Wastewater Treatment
For certain acid mine wastewater, a concentration of stibium is 14.876 m/L and a pH of wastewater is 2.7. Take 1 L wastewater, add 0.1 g titanium hexametaphosphate adsorbent-2 prepared in Embodiment 2, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of stibium in the wastewater by an ICP-MS method, the concentration of stibium in wastewater measured being 2.345 μg/L.
Contrast Embodiment 1: A Titanium Dioxide Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 2.157 mg/L and a pH of wastewater is 2.7. Take 1 L wastewater, add 0.8 g titanium dioxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium in wastewater measured being 0.205 mg/L.
Contrast Embodiment 2: A Manganese Dioxide Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 5.029 mg/L and a pH of wastewater is 3.5. Take 1 L wastewater, add 0.5 g manganese dioxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.183 mg/L and the concentration of manganese being 1.211 mg/L (material dissolved).
Contrast Embodiment 3: A Hydrated Ferric Oxide Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 4.121 mg/L and a pH of wastewater is 3.0. Take 1 L wastewater, add 0.6 g hydrated ferric oxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.335 mg/L and the concentration of ferri being 2.19 mg/L (material dissolved).
Contrast Embodiment 4: An Aluminum Oxide Adsorbent in Wastewater Treatment
For certain thallium-containing wastewater, a concentration of univalent thallium is 6.923 mg/L and a pH of wastewater is 2.7. Take 1 L wastewater, add 0.8 g aluminum oxide adsorbent, perform solid-liquid separation after stirring and mixing for 1 h, and measure a concentration of thallium in the wastewater by an ICP-MS method, the concentration of thallium measured being 0.818 mg/L and the concentration of aluminum being 0.819 mg/L (material dissolved).

Claims (5)

What is claimed:
1. A method for producing an absorbent, comprising:
adding acid into a hexametaphosphate solution for adjusting a pH to prepare a mixed solution, wherein the hexametaphosphate is selected from a group consisting of sodium hexametaphosphate, potassium hexametaphosphate, and ammonium hexametaphosphate,
adding titanium salt into the mixed solution,
reacting, aging and filtering to obtain a filter residue as the absorbent.
2. The method of claim 1, wherein, the pH is 0-6; preferably, the pH is 0-3.
3. The method of claim 1, wherein a ratio of amount of substance of the hexametaphosphate to the titanium salt is (1-2):(3-1).
4. The method of claim 1, wherein, the titanium salt is selected from at least one of titanium tetrachloride, titanium oxychloride, titanium nitrate or titanium sulfate.
5. The method of claim 1, further comprising purifying of a filter residue; wherein the purifying includes water washing and drying.
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